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Method for reaction rectification coupling continuous preparation of and series acetate

A series of esters and acetic acid technology, applied in the field of continuous preparation of acetic acid series esters, can solve the problem of low conversion rate of esters

Active Publication Date: 2006-09-27
GUANGXI RES INST OF CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lan Pingping [Hebei Chemical Industry. 1997, (3): 46] has carried out research with strong acid type cation exchange resin catalytic synthesis ethyl acetate, adopts intermittent stirring mode, and the conversion rate of ester is 64.21%, and the conversion rate of this method ester is too low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Catalyst preparation

[0034] Put hydrogen type D001 macroporous strongly acidic styrene-based cation exchange resin into 0.1-1.5% cerium nitrate solution, the volume ratio of ion-exchange resin to solution is 1:3, at a temperature of 50-55°C and -0.05-- Under a vacuum of 0.06MPa, soak for 8 hours, filter out the cerium nitrate solution, and repeat the treatment 2 to 3 times under the same conditions. In the same way, treat the ion exchange resin with 0.2% zirconium nitrate solution, then wash it with deionized water until there is no chloride ion, and dry it at a temperature of 110-120°C and a vacuum of -0.09--0.095MPa , prepared a modified D001 hydrogen-type strongly acidic styrene-based cation exchange resin catalyst.

Embodiment 2

[0036] Put the hydrogen type 001×7 strongly acidic styrene-based cation exchange resin into 0.1% cerium nitrate solution, the volume ratio of the ion exchange resin to the solution is 1:3, at a temperature of 50~55°C and -0.05~-0.06MPa Under a certain vacuum degree, soak for 11 hours, filter off the cerium nitrate solution, and repeat the treatment 2 to 3 times under the same conditions. In the same way, the ion exchange resin is treated with 0.2% zirconium nitrate solution, then washed with deionized water until there is no chloride ion, and dried at a temperature of 100°C and a vacuum of -0.09 to -0.095MPa to prepare A modified 001×7 hydrogen type strongly acidic styrene-based cation exchange resin catalyst was produced.

Embodiment 3

[0038] Preparation of ethyl acetate

[0039] The modified D001 hydrogen type strongly acidic styrenic cation exchange resin catalyst 30 grams prepared in embodiment 1 is to pack in the fluidized bed reactor of 25mm, length 500mm, then add 130g glacial acetic acid. Add 800g of glacial acetic acid to the rectification tower kettle with an inner diameter of 25mm, a rectification section of 800mm and a stripping section of 500mm, and control the temperature of the fluidized bed reactor at about 85°C and the temperature of the rectification tower at about 118°C. Mix glacial acetic acid and 95% ethanol in a molar ratio of 1:1, and enter the fluidized bed reactor at a rate of 150ml / h, and extract the still liquid from the rectification column tank to enter the fluidized bed at a rate of 150-250ml / h In the reactor, adjust the circulation speed of the kettle liquid within the speed range to make the catalyst fluidized, and the glacial acetic acid and ethanol undergo a fluidized catalyt...

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Abstract

The invention discloses a reaction-distillation coupling preparing acetic acid series ester method, which comprises the following steps: using glacial acetic acid and alcohol with lower five carbons (alcohol, optal,alcohol isopropylicum, butanol, isobutanol, amyl alcohol and isoamyl alcohol ) for raw material; adopting modified strong acidic phenylethene series basic ion exchange resin for accelerant; preparing by reaction-distillation coupling; getting acetic acid ethyl ester, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, amyl acetate and iso-amyl acetate; making glacial acetic acid and alcohol with lower five carbons to carry on esterification reaction by solid acid catalysis in trickle bed reactor; adding reaction product (acetic acid ethyl ester, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, amyl acetate and iso-amyl acetate), water and cycle still liquor in fractionating tower; getting acetic acid ethyl ester, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, amyl acetate and iso-amyl acetate by separating at the top of the tower. The conversion rate of alcohol with lower five carbons is more than 96%, the recovery ratio of acetic acid ethyl ester (propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, amyl acetate and iso-amyl acetate) is more than 95%. The invention has high alcohol conversion rate, which simplifies the operation.

Description

technical field [0001] The invention relates to a method for continuously preparing acetic acid series esters. More specifically, it relates to a method for continuously preparing acetic acid series esters by using a modified cation exchange resin as a catalyst through reaction-distillation coupling. Background technique [0002] Ethyl acetate is a colorless transparent liquid, miscible with organic solvents such as ethanol, ether, chloroform, benzene, acetone, and slightly soluble in water. Ethyl acetate is widely used as a solvent for paints, varnishes, artificial leather, nitrocellulose, vinyl acetate, etc., as well as an extraction agent for drugs and organic acids. In recent years, it has been developed as an adhesive and bioaccelerator, and can be used as a raw material for dyes, pharmaceuticals, and chemicals. Ethyl acetate can also be used as a food flavor. [0003] Isopropyl acetate is a fine chemical raw material, which is mainly used as an extraction solvent fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08B01J31/08
Inventor 黄科林黄焕生樊晓丹罗素娟王桂英卢军
Owner GUANGXI RES INST OF CHEM IND CO LTD
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